KR940005539B1 - Process for producing receding of water agent of mortar and concrete - Google Patents
Process for producing receding of water agent of mortar and concrete Download PDFInfo
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- KR940005539B1 KR940005539B1 KR1019910016266A KR910016266A KR940005539B1 KR 940005539 B1 KR940005539 B1 KR 940005539B1 KR 1019910016266 A KR1019910016266 A KR 1019910016266A KR 910016266 A KR910016266 A KR 910016266A KR 940005539 B1 KR940005539 B1 KR 940005539B1
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- South Korea
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- reducing agent
- water reducing
- concrete
- mortar
- naphthol
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
- C04B22/14—Acids or salts thereof containing sulfur in the anion, e.g. sulfides
Abstract
Description
본 발명은 나프톨을 황산화한 후 이를 포르말린으로 축합시킨 축합물 또는 그 중성화물을 주성분으로 하는 몰탈 및 콘크리트용 비공기연행성 감수제의 제조방법 및 그 감수제에 관한 것이다.The present invention relates to a method for producing a mortar and concrete non-air-conducting water reducing agent mainly containing a condensate obtained by sulfating naphthol and condensing it with formalin or a neutralized product thereof, and a water reducing agent.
일반적으로 고성능 감수제는 강력한 시멘트 분산작용을 하므로 콘크리트를 제조할 때 첨가하면 콘크리트의 유동성이 향상되어 시공시에 콘크리트 이송작업이 보다 용이하게 되고 물을 적게 사용하여도 되므로 용수가 절약될뿐 아니라 콘크리트의 강도증대와 균열감소등의 품질개선효과가 크기 때문에 석고, 몰탈, 콘크리트등의 제조시에 널리 사용되고 있다.In general, high-performance water reducing agents have a strong cement dispersion effect, so adding them in the manufacture of concrete improves the fluidity of the concrete, making it easier to transport the concrete during construction and using less water. It is widely used in the manufacture of gypsum, mortar, concrete, etc. because of its quality improvement effect such as strength increase and crack reduction.
특히 콘크리트의 유동성은 콘크리트의 이송작업이 용이하도록 하므로서 각종 공기의 단축은 물론 이송장비의 마모가 적어 사용수명이 길어지고 또한 이송시의 에너지 절약효과도 얻을 수 있어 콘크리트의 유동성을 보다 향상케하는 감수제의 발명은 매우 중요한 것이다.In particular, the fluidity of concrete facilitates the conveying work of concrete, which shortens the air and reduces the wear of the conveying equipment, resulting in a long service life and an energy saving effect during conveying. The invention is very important.
종래 이러한 감수제로서는 나프탈렌술폰산 단독화합물을 포름알데히드에 의하여 축합한 축합물(일본특허공개소61-83659호)이나 술폰화한 멜라민의 포름알데히드 축합물 또는 리그닌술폰산 나트륨염이 사용되고 있다.Conventionally, as such a water reducing agent, the condensate which condensed a naphthalene sulfonic acid homogeneous compound with formaldehyde (Japanese Patent Publication No. 61-83659), the formaldehyde condensate of sulfonated melamine, or the lignin sulfonic acid sodium salt is used.
본 발명은 이러한 종래 감수제보다 콘크리트의 유동성이 더욱 높은 우수한 감수제를 제공하기 위한 것이다.The present invention is to provide an excellent water reducing agent having a higher fluidity of concrete than such a conventional water reducing agent.
여러 가지로 시험분석한바 나프톨술폰산에는 수용성 분산력을 나타내는 술폰산나트륨외에 시멘트입자 및 물과의 수소결합력을 갖는 수산기(-OH)가 있어 수중에서 시멘트 입자를 분산시키는 효과가 매우 크다는 것을 알았고 이러한 나프톨술폰산을 포름알데히드로 축합시킨 고축합물을 감수제로 사용할 경우 시멘트의 유동성이 더욱 뛰어나게 된다는 것을 알았다.The naphthol sulfonic acid was found to have a very high effect of dispersing cement particles in water because the naphthol sulfonic acid had a hydroxyl group (-OH) having a hydrogen bonding force between cement particles and water in addition to sodium sulfonic acid, which exhibits water-soluble dispersibility. It was found that when the high-condensation product condensed with formaldehyde was used as a water reducing agent, the fluidity of the cement was better.
본 발명 감수제의 제조방법은 다음과 같다.The manufacturing method of the water reducing agent of the present invention is as follows.
나프톨을 황산화 하여서된 나프톨술폰산에 포름알데히드를 첨가하여 60。-90℃에서 10-20시간 반응시킨 다음 반응액에 수산화칼슘이나 수산화마그네슘 등을 투입하여 미반응 황산을 침석시키므로서 불용성을 분리하고 불용분(침석물)이 분리된 반응액에 가성소다등의 염기성 물질을 적량투입하여 반응액을 PH 7-9로 조절 중성화하므로서 본 발명의 감수제 제조가 완성된다.Formaldehyde was added to naphtholsulfonic acid obtained by sulfated naphthol and reacted at 60 ° -90 ° C for 10-20 hours, and then calcium hydroxide or magnesium hydroxide was added to the reaction solution to precipitate unreacted sulfuric acid, thereby insoluble and insoluble. Preparation of the water sensitizer of the present invention is completed by controlling and neutralizing the reaction solution to pH 7-9 by appropriately introducing basic substances such as caustic soda into the reaction solution from which the powders (sediments) are separated.
본 발명의 실시예를 공정별로 상세히 설명하면 다음과 같다.An embodiment of the present invention will be described in detail by process.
[실시예]EXAMPLE
[제1공정(황산화공정)][Step 1 (Sulfate Oxidation)]
나프톨 72g을 120℃로 가열용해하고 120℃에서 98% 황산 57g을 넣으면서 약 2시간정도 가열하고 다시 140℃로 승온시켜 약 3시간동안 반응후 약 70℃까지 냉각되게 한다.After heating and dissolving 72 g of naphthol at 120 ° C., 57 g of 98% sulfuric acid at 120 ° C. was heated for about 2 hours, and the temperature was raised to 140 ° C., and then cooled to about 70 ° C. after the reaction for about 3 hours.
[제2공정(축합공정)]Second Process (Condensation Process)
제1공정에서 황산화된 나프톨(나프톨술폰산)은 대체로 점도가 높기 때문에 증류수를 첨가하여 적절한 수용액으로 한 후 이 수용액에 포름알데히드(37% 포르말린 수용액) 56g을 투입하고 80℃에서 10-20시간 반응시키고 통상의 방법으로 분석하여 반응이 90%이상이면 반응을 종결한다.Since naphthol (naphtholsulfonic acid) sulfated in the first step is generally high in viscosity, distilled water is added to an appropriate aqueous solution, and 56 g of formaldehyde (37% formalin aqueous solution) is added thereto and reacted at 80 ° C for 10-20 hours. The reaction is terminated when the reaction is 90% or more by analyzing in a conventional manner.
[제3공정(불용분 분리 및 중화공정)][3rd process (Insoluble matter separation and neutralization process)]
제2공정에서 얻은 반응액의 점도가 높을 경우에는 소량의 물을 첨가하여 적절히 회석한 다음 수산화칼슘 7.4g과 물 17g을 첨가하여 미반응 황산을 염으로 침석시키고 침석된 염(불용분)을 분리제거하여 순수한 반응액을 얻고 이 반응액에 가성소다 수용액을 넣어 중화(PH 7-9)하므로서 본 발명이 완성된다.If the reaction solution obtained in the second step has a high viscosity, a small amount of water is added to the mixture, and the reaction is appropriately diluted. Then, 7.4 g of calcium hydroxide and 17 g of water are added to precipitate the unreacted sulfuric acid as a salt and the precipitated salt (insoluble content) is separated and removed. The reaction solution was obtained by neutralization (PH 7-9) by adding a caustic soda solution to the reaction solution, thereby completing the present invention.
반응액을 중화시켜서 된 액상의 감수제를 그대로 사용하거나 또는 분무건조하여 분말상의 감수제로 하여도 된다.You may use the liquid water reducing agent which neutralized the reaction liquid as it is, or spray-drying it as a powdery water reducing agent.
분말상의 감수제는 액상의 감수제보다 보관이나 운반등이 용이하거나 사용시에는 다시 물에 넣어 액화하므로 그 작용효과는 서로 같다.Powdered water reducing agents are easier to store and transport than liquid water reducing agents, or when used, they are liquefied into water and used again, so the effect is the same.
이와 같이 제조된 본 발명의 감수제는 대체로 시멘트에 대하여 0.01%-5%의 중량비로 투입사용하며 아래와 같은 방법으로 시험한바 본 발명 감수제의 작용효과는 (표1)과 같다.The water reducing agent of the present invention prepared as described above is generally used in a weight ratio of 0.01% -5% with respect to cement and tested by the following method, and the effect of the present water reducing agent is shown in Table 1 below.
시험방법 : 본 발명의 감수제와 종래의 감수제를 각각 일정비율로 시멘트몰탈과 혼합반죽하여 원통형 플로우측정기(높이 5㎝, 상부직경 7㎝, 하부직경 10㎝)에 다져넣고 1분후 몰드를 들어올린 다음에 시멘트몰탈이 놓인 원판을 15초동안 25회 회전시키고 그때 흘려내린 시멘트몰탈의 지름을 4방향에서 측정하여 그 평균값을 슬럼프값으로 하였다.Test method: Mixing and mixing the water reducing agent of the present invention and the conventional water reducing agent with a cement mortar at a predetermined ratio, put into a cylindrical flow measuring device (height 5cm, upper diameter 7cm, lower diameter 10cm) and lifted the mold after 1 minute The disc on which the cement mortar was placed was rotated 25 times for 15 seconds, and the diameter of the cement mortar which had flowed out at that time was measured in four directions, and the average value was taken as the slump value.
압축강도는 시멘트몰탈을 4㎝×4㎝×16㎝ 규격의 3연 몰드에 성형하여 28일간 수중 양생한 후 만능시험기를 이용하여 JIS 기준에 의거 실험한 것이다.Compressive strength is a cement mortar was molded into a three-mould mold of the 4cm × 4cm × 16cm standard and cured in water for 28 days, and then tested according to JIS standard using a universal testing machine.
(본 시험 사용 시멘트는 포트랜드시멘트이고 모래는 강모래임)(The cement used in this test is Portland cement and sand is steel sand.)
[표 1]TABLE 1
표(1)에서 종래 감수제(1)은 나프탈렌술폰산 단독화합물을 포름알데히드에 의하여 축합한 것In Table (1), the conventional water reducing agent (1) is a condensation of naphthalene sulfonic acid homo-compound with formaldehyde.
종래 감수제(2)는 리그닌술폰산 나트륨염을 그대로 사용한 것Conventional water reducing agent (2) using the lignin sulfonic acid sodium salt as it is
기타는 감수제를 사용하지 아니한 것이다.Others do not use water reducing agents.
이상 표(1)에서 알 수 있는 바와 같이 감수제를 첨가하지 아니한 시멘트몰탈의 슬럼프가 11.1㎝임에 비하여 나프탈렌술폰산 축합물염을 사용한 종래 감수제(1)의 경우에는 15.9㎝으로서 약 43.2%의 상승효과가 있고 이에 비하여 본 발명을 첨가한 것은 17.9㎝으로서 약 61.3%의 상승효과가 있음을 알 수 있으며 압축강도에 있어서는 종래 감수제(1)이 389㎏/㎠이고 본 발명은 382㎏/㎠로서 거의 대등한 강도를 나타내고 있어 본 발명의 감수제가 종래보다 유동성이 뛰어난 것임을 알 수 있다.As can be seen from the above table (1), the slump of the cement mortar without the addition of the water reducing agent is 11.1 cm, whereas the conventional water reducing agent (1) using naphthalene sulfonic acid condensate salt has a synergistic effect of about 43.2%. On the other hand, the addition of the present invention was found to have a synergistic effect of about 61.3% as 17.9cm, and the conventional water reducing agent (1) was 389㎏ / ㎠ and the present invention was almost equivalent to 382㎏ / ㎠. It demonstrates strength and shows that the water reducing agent of this invention is excellent in fluidity | liquidity conventionally.
따라서 본 발명의 감수제는 시멘트몰탈의 유동성을 보다 향상시키므로서 시공이 더욱 신속용이하여 각종 공기가 단축되고 장비의 사용수명이 길어지며 이송에너지가 절감되는 효과가 있는 것이다.Therefore, the water reducing agent of the present invention is to improve the fluidity of the cement mortar more easily, the construction is more easy to shorten the various air, the service life of the equipment is long and the transfer energy is reduced.
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KR1019910016266A KR940005539B1 (en) | 1991-09-16 | 1991-09-16 | Process for producing receding of water agent of mortar and concrete |
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KR940005539B1 true KR940005539B1 (en) | 1994-06-20 |
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KR100402175B1 (en) * | 2000-11-16 | 2003-10-17 | 주식회사 우성에퍼트코리아 | Lubricant products for spining in textile industry |
KR101010291B1 (en) * | 2010-09-17 | 2011-01-25 | 김정수 | Ecological self-cleaning knitting/coning oil compsition and method therefor |
KR102249081B1 (en) | 2020-08-28 | 2021-05-10 | 아이씨이아이우방(주) | Spinning oil composition for polyester industrial yarns, Spinning oil using the same and Manufacturing method thereof |
KR102576568B1 (en) | 2021-11-10 | 2023-09-08 | 아이씨이아이우방(주) | Spinning oil composition for polyester full draw yarns, Spinning oil using the same and Manufacturing method thereof |
KR20230105447A (en) | 2022-01-04 | 2023-07-11 | 아이씨이아이우방(주) | Spinning oil composition for polyester bulked continuous filament, Spinning oil using the same and Manufacturing method thereof |
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